TATB制备废水中污染物成分的分离分析研究

发布时间：2018-03-07 09:09

本文选题：TATB废水　切入点：液相色谱-质谱联用　出处：《南京理工大学》2017年硕士论文　论文类型：学位论文

【摘要】：1,3,5-三氨基-2,4,6-三硝基苯(TATB)是一种高能钝感炸药,也是最早的耐热炸药之一,广泛应用于军事民用等各个领域,其合成过程中三个阶段产生大量有机废水,色谱法是目前应用最广泛的废水分析方法。本文采用液质联用(LC-MS)、高效液相色谱(HPLC)、气相色谱(GC)等色谱仪器对TATB制备废水中有机污染物成分进行分析鉴定,采用液液萃取、固相萃取等前处理手段对废水进行处理得到固体物质,采用红外(IR)、核磁(NMR)以及高分辨质谱(HRMS)等分析仪器对其进行表征,建立相应的分析方法。采用液相色谱-质谱联用(LC-MS)对废水中的难挥发性物质进行分析鉴定,结合线性离子阱-傅里叶变换质谱(LTQ-FT-MS)对组分进行定性分析,确定了废水中热不稳定及难挥发性组分的成分组成;对废水进行处理得到固体物质,采用红外、核磁以及高分辨质谱进行表征确定其结构,从硝化废水中得到1,3,5-三羟基-2,4,6-三硝基苯(TNPG)固体,对胺化废水进行过柱重结晶分得到1,3,5-三乙氧基-2,4,6-三硝基苯(TETNB)和1-氨基-3,5-二乙氧基-2,4,6-三硝基苯;采用HPLC对TATB废水中4种苯类衍生物进行分析,得出了各阶段废水中四种苯类衍生物的含量,建立了 TATB废水中4种物质的HPLC分析方法;采用气相色谱对废水中的乙醇、丙酮、原甲酸三乙酯等小分子物质的含量进行测定,得出了各废水中小分子的含量,建立了相应的气相色谱分析方法,适用于工业废水体系中小分子残留的分析。
[Abstract]:1,3,5- -2,4,6- three amino three nitrobenzene (TATB) is a kind of insensitive high explosives, one of heat-resistant explosives is also one of the earliest and widely used in military and civil fields, a large number of organic wastewater from the three stages of the synthesis process, wastewater chromatography is currently the most widely used analytical method. By using liquid chromatography-mass spectrometry (LC-MS), high performance liquid chromatography (HPLC), gas chromatography (GC) and other chromatographic instruments on the preparation of TATB organic pollutants in wastewater were analyzed and identified, using liquid-liquid extraction, solid phase extraction pretreatment method for processing the solid matter of wastewater, using infrared (IR), nuclear magnetic resonance (NMR) and high resolution mass spectrometry (HRMS) was characterized as analytic instrument, establish corresponding analysis method. By using liquid chromatography-mass spectrometry (LC-MS) were identified in the wastewater to volatile substances, combined with linear ion trap Fourier transform mass spectrometry (LTQ- FT-MS) were divided to group qualitative analysis, composition of wastewater heat labile and difficult volatile ingredients were determined; processing of solid material for wastewater by IR, NMR and high resolution mass spectrometry to determine its structure was characterized by 1,3,5-, -2,4,6- three hydroxy three nitrobenzene from nitrification in wastewater (TNPG) on solid. A column of amination wastewater recrystallization points 1,3,5- triethoxy -2,4,6- three nitrobenzene (TETNB) and 1- -3,5- two amino ethoxy -2,4,6- three nitrobenzene; using HPLC analysis of 4 kinds of benzene derivatives in TATB wastewater, the contents of four kinds of benzene derivatives in various stages of wastewater, set up 4 kinds of material TATB HPLC in the wastewater analysis method; chromatography in the wastewater by gas ethanol, acetone, ethyl formate content of three molecules were determined, the content of the wastewater of small molecules, established the corresponding The analytical method of gas chromatography is suitable for the analysis of small and medium molecular residues in industrial wastewater.

【学位授予单位】：南京理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.63;X832

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